関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 4-Chlorobutyryl chloride | HCID 78370 | — |
| 反応物 | 2-[(2-Aminoethyl)disulfanyl]ethan-1-amine hydrochloride | HCID 167628 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N,N'-(disulfanediyldiethane-2,1-diyl)bis(4-chlorobutanamide) | HCID 10666287 | — |
反応手順
60 g of cystamine hydrochloride was solubilized in 500 mL and cooled to 5° C. The pH was raised to 10 by addition of aq. NaOH (30%). A solution of 4-chlorobutanoyl chloride (105 g) in anhydrous THF (500 mL), was added dropwise, while the pH was maintained above 7 by addition of aq. NaOH (30%). After completion of the addition and stabilization of pH at 7, the mixture mixed for 3 days. The aqueous layer was extracted with 3×500 mL dichloromethane, combined with THF layer and dried over Na2SO4. After drying under vacuum, 41 g of a white powder were collected. Analyses were in accordance with the expected structure.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07717964B2 |
|---|
| 出典データセット | uspto-grants-2010_05 |
|---|
| ORD ID | ord-0c79e47db59f4b84a45a00062d668bae |
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| 出典メモ | uspto-grants-2010_05 |
|---|
